data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Vadim G. Kessler' 'Fernand Chassagneux' 'Stephane Parola' 'Martine Verdenelli' 'Pia Werndrup' _publ_contact_author_name 'Dr Vadim G. Kessler' _publ_contact_author_address ; Department of Chemistry Swedish University of Agricultural Sciences Box 7015 Uppsala 75007 SWEDEN ; _publ_contact_author_email VADIM.KESSLER@KEMI.SLU.SE _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Mesoporous Powders and Dense Thin Films of Late Transition Metal Oxide Nanocomposites from Structurally Characterized Single-Source Precursors ; data_cotaet1m _database_code_depnum_ccdc_archive 'CCDC 212056' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H37 Co O8 Ta' _chemical_formula_weight 609.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.814(3) _cell_length_b 11.804(3) _cell_length_c 12.086(3) _cell_angle_alpha 69.327(4) _cell_angle_beta 85.781(4) _cell_angle_gamma 70.693(4) _cell_volume 1234.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3670(I>2sigma(I)) _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 5.133 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2333 _exptl_absorpt_correction_T_max 0.3081 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3758 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.1244 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 20.00 _reflns_number_total 2274 _reflns_number_gt 1487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2274 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.32087(9) 0.19904(8) 0.30347(7) 0.0729(4) Uani 1 1 d . . . Co1 Co 0.4093(2) 0.0745(2) 0.59059(19) 0.0658(7) Uani 1 1 d . . . O1 O 0.2692(16) 0.3590(14) 0.3088(13) 0.120(6) Uani 1 1 d . . . O6 O 0.3953(12) 0.0193(13) 0.3128(11) 0.088(4) Uani 1 1 d . . . O3 O 0.4161(14) 0.2436(14) 0.1663(14) 0.109(5) Uani 1 1 d . . . O4 O 0.2447(12) 0.1354(12) 0.4652(10) 0.091(4) Uani 1 1 d . . . O2 O 0.1444(13) 0.2157(13) 0.2367(11) 0.103(4) Uani 1 1 d . . . O5 O 0.5104(10) 0.1217(12) 0.4147(9) 0.083(4) Uani 1 1 d . . . O7 O 0.3775(13) 0.2453(12) 0.6056(12) 0.078(4) Uani 1 1 d . . . C13 C 0.304(3) 0.290(2) 0.679(2) 0.084(6) Uani 1 1 d . . . C9 C 0.622(2) 0.178(2) 0.410(2) 0.113(8) Uani 1 1 d . . . C11 C 0.105(3) 0.119(3) 0.501(2) 0.128(9) Uani 1 1 d . . . H11A H 0.0666 0.0951 0.4436 0.154 Uiso 1 1 calc R . . H11B H 0.1154 0.0521 0.5775 0.154 Uiso 1 1 calc R . . C14 C 0.221(2) 0.100(3) 0.7893(19) 0.085(7) Uani 1 1 d . . . C15 C 0.299(3) 0.424(2) 0.668(2) 0.155(11) Uani 1 1 d . . . H15A H 0.3564 0.4555 0.6047 0.233 Uiso 1 1 calc R . . H15B H 0.3357 0.4215 0.7411 0.233 Uiso 1 1 calc R . . H15C H 0.2005 0.4807 0.6528 0.233 Uiso 1 1 calc R . . C5 C 0.496(4) 0.235(3) 0.065(3) 0.200(17) Uani 1 1 d . . . H5A H 0.5984 0.2034 0.0866 0.241 Uiso 1 1 calc R . . H5B H 0.4752 0.1730 0.0388 0.241 Uiso 1 1 calc R . . C7 C 0.362(3) -0.028(2) 0.209(3) 0.149(13) Uani 1 1 d . . . H7A H 0.3063 0.0441 0.1428 0.179 Uiso 1 1 calc R . . H7B H 0.4509 -0.0736 0.1811 0.179 Uiso 1 1 calc R . . C12 C 0.010(3) 0.238(3) 0.506(2) 0.172(13) Uani 1 1 d . . . H12A H -0.0841 0.2304 0.5264 0.257 Uiso 1 1 calc R . . H12B H 0.0024 0.3037 0.4299 0.257 Uiso 1 1 calc R . . H12C H 0.0468 0.2589 0.5645 0.257 Uiso 1 1 calc R . . C2 C 0.208(4) 0.571(3) 0.262(3) 0.218(17) Uani 1 1 d . . . H2A H 0.1503 0.6357 0.2932 0.327 Uiso 1 1 calc R . . H2B H 0.1667 0.5863 0.1868 0.327 Uiso 1 1 calc R . . H2C H 0.3046 0.5739 0.2539 0.327 Uiso 1 1 calc R . . C8 C 0.295(3) -0.096(3) 0.257(3) 0.204(18) Uani 1 1 d . . . H8A H 0.2693 -0.1285 0.2014 0.306 Uiso 1 1 calc R . . H8B H 0.2088 -0.0494 0.2851 0.306 Uiso 1 1 calc R . . H8C H 0.3521 -0.1664 0.3220 0.306 Uiso 1 1 calc R . . C1 C 0.209(6) 0.467(4) 0.330(4) 0.32(4) Uani 1 1 d . . . H1A H 0.1090 0.4735 0.3455 0.389 Uiso 1 1 calc R . . H1B H 0.2544 0.4552 0.4037 0.389 Uiso 1 1 calc R . . C10A C 0.588(4) 0.311(4) 0.375(3) 0.12(2) Uiso 0.62(6) 1 d P . . C10B C 0.663(5) 0.250(5) 0.309(5) 0.07(2) Uiso 0.38(6) 1 d P . . O8 O 0.2864(13) 0.0324(13) 0.7302(12) 0.083(4) Uani 1 1 d . . . C16 C 0.227(2) 0.223(3) 0.767(2) 0.103(7) Uani 1 1 d . . . H16A H 0.1740 0.2664 0.8160 0.124 Uiso 1 1 calc R . . C17 C 0.126(3) 0.054(2) 0.885(2) 0.149(10) Uani 1 1 d . . . H17A H 0.1309 -0.0312 0.8924 0.224 Uiso 1 1 calc R . . H17B H 0.0278 0.1101 0.8647 0.224 Uiso 1 1 calc R . . H17C H 0.1574 0.0534 0.9582 0.224 Uiso 1 1 calc R . . C6 C 0.468(5) 0.335(4) -0.015(4) 0.28(3) Uani 1 1 d . . . H6A H 0.5234 0.3241 -0.0817 0.419 Uiso 1 1 calc R . . H6B H 0.4917 0.3959 0.0093 0.419 Uiso 1 1 calc R . . H6C H 0.3668 0.3666 -0.0373 0.419 Uiso 1 1 calc R . . C4 C -0.050(6) 0.295(9) 0.120(5) 0.28(3) Uani 1 1 d . . . C3A C 0.021(8) 0.372(8) 0.132(5) 0.20(4) Uiso 0.65(15) 1 d P . . C3B C 0.059(16) 0.267(12) 0.112(9) 0.16(7) Uiso 0.35(15) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.0670(6) 0.0779(7) 0.0677(6) -0.0199(4) -0.0100(4) -0.0191(4) Co1 0.0591(16) 0.0771(18) 0.0660(17) -0.0297(13) -0.0008(13) -0.0224(13) O1 0.128(12) 0.070(11) 0.108(12) -0.007(9) -0.015(9) 0.013(9) O6 0.049(7) 0.130(11) 0.085(9) -0.036(8) -0.018(7) -0.027(7) O3 0.073(10) 0.132(12) 0.121(13) -0.060(10) 0.004(9) -0.016(8) O4 0.047(8) 0.135(11) 0.078(9) -0.016(8) -0.011(7) -0.032(7) O2 0.081(9) 0.135(12) 0.098(10) -0.021(9) -0.027(8) -0.056(8) O5 0.033(7) 0.144(11) 0.058(7) -0.031(7) -0.007(6) -0.015(7) O7 0.070(9) 0.081(10) 0.082(10) -0.035(8) -0.005(7) -0.014(7) C13 0.081(17) 0.087(19) 0.092(18) -0.045(15) -0.026(14) -0.019(14) C9 0.078(15) 0.099(19) 0.17(2) -0.006(15) -0.036(15) -0.073(14) C11 0.11(2) 0.17(3) 0.099(19) -0.042(18) -0.032(17) -0.05(2) C14 0.052(14) 0.12(2) 0.076(17) -0.020(16) -0.003(12) -0.032(14) C15 0.22(3) 0.09(2) 0.14(2) -0.036(16) -0.02(2) -0.027(19) C5 0.17(3) 0.16(3) 0.18(4) -0.03(3) 0.00(3) 0.03(3) C7 0.10(2) 0.069(19) 0.22(4) 0.014(19) -0.04(2) -0.023(15) C12 0.11(2) 0.25(4) 0.11(2) -0.06(2) -0.020(17) 0.00(2) C2 0.28(4) 0.16(3) 0.20(4) -0.04(3) 0.04(3) -0.07(3) C8 0.14(3) 0.17(4) 0.24(4) 0.00(3) 0.00(3) -0.05(2) C1 0.48(8) 0.15(4) 0.18(4) 0.02(3) 0.04(5) 0.00(5) O8 0.068(9) 0.098(10) 0.084(10) -0.042(8) 0.003(7) -0.017(7) C16 0.092(18) 0.11(2) 0.11(2) -0.066(17) 0.009(15) -0.019(16) C17 0.16(2) 0.16(2) 0.11(2) -0.045(17) 0.049(19) -0.046(19) C6 0.31(6) 0.21(4) 0.22(5) 0.03(3) 0.02(4) -0.07(4) C4 0.15(4) 0.39(7) 0.35(6) -0.15(5) -0.01(4) -0.14(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 O1 1.810(16) . ? Ta1 O3 1.838(17) . ? Ta1 O2 1.886(12) . ? Ta1 O6 1.967(14) . ? Ta1 O4 2.015(12) . ? Ta1 O5 2.116(10) . ? Co1 O8 2.013(14) . ? Co1 O7 2.008(14) . ? Co1 O6 2.068(11) 2_656 ? Co1 O4 2.061(12) . ? Co1 O5 2.209(13) 2_656 ? Co1 O5 2.244(11) . ? O1 C1 1.32(5) . ? O6 C7 1.63(4) . ? O6 Co1 2.068(11) 2_656 ? O3 C5 1.42(4) . ? O4 C11 1.46(2) . ? O2 C3B 1.59(12) . ? O2 C3A 1.89(6) . ? O5 C9 1.44(2) . ? O5 Co1 2.209(13) 2_656 ? O7 C13 1.25(2) . ? C13 C16 1.42(3) . ? C13 C15 1.53(3) . ? C9 C10B 1.34(5) . ? C9 C10A 1.41(4) . ? C11 C12 1.42(3) . ? C14 O8 1.25(3) . ? C14 C16 1.41(3) . ? C14 C17 1.49(3) . ? C5 C6 1.20(3) . ? C7 C8 1.17(3) . ? C2 C1 1.20(4) . ? C10A C10B 1.30(5) . ? C4 C3B 1.02(11) . ? C4 C3A 1.36(8) . ? C3A C3B 1.27(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ta1 O3 92.1(7) . . ? O1 Ta1 O2 97.2(7) . . ? O3 Ta1 O2 98.7(6) . . ? O1 Ta1 O6 173.0(6) . . ? O3 Ta1 O6 89.5(6) . . ? O2 Ta1 O6 89.3(5) . . ? O1 Ta1 O4 90.7(6) . . ? O3 Ta1 O4 171.8(5) . . ? O2 Ta1 O4 88.5(5) . . ? O6 Ta1 O4 86.9(5) . . ? O1 Ta1 O5 96.5(6) . . ? O3 Ta1 O5 94.1(5) . . ? O2 Ta1 O5 160.8(5) . . ? O6 Ta1 O5 76.6(5) . . ? O4 Ta1 O5 77.9(4) . . ? O8 Co1 O7 89.4(5) . . ? O8 Co1 O6 95.5(5) . 2_656 ? O7 Co1 O6 96.4(5) . 2_656 ? O8 Co1 O4 95.0(5) . . ? O7 Co1 O4 96.8(5) . . ? O6 Co1 O4 163.2(5) 2_656 . ? O8 Co1 O5 94.9(5) . 2_656 ? O7 Co1 O5 168.5(4) . 2_656 ? O6 Co1 O5 72.5(5) 2_656 2_656 ? O4 Co1 O5 93.5(5) . 2_656 ? O8 Co1 O5 168.7(5) . . ? O7 Co1 O5 94.9(5) . . ? O6 Co1 O5 94.5(4) 2_656 . ? O4 Co1 O5 74.2(4) . . ? O5 Co1 O5 83.0(5) 2_656 . ? C1 O1 Ta1 167(3) . . ? C7 O6 Ta1 122.9(11) . . ? C7 O6 Co1 119.3(12) . 2_656 ? Ta1 O6 Co1 110.6(6) . 2_656 ? C5 O3 Ta1 160.6(19) . . ? C11 O4 Ta1 130.9(12) . . ? C11 O4 Co1 120.3(11) . . ? Ta1 O4 Co1 108.6(5) . . ? C3B O2 Ta1 141(5) . . ? C3B O2 C3A 42(4) . . ? Ta1 O2 C3A 124(3) . . ? C9 O5 Ta1 127.6(11) . . ? C9 O5 Co1 114.2(12) . 2_656 ? Ta1 O5 Co1 100.1(5) . 2_656 ? C9 O5 Co1 114.1(12) . . ? Ta1 O5 Co1 98.7(4) . . ? Co1 O5 Co1 97.0(5) 2_656 . ? C13 O7 Co1 128.0(15) . . ? O7 C13 C16 124(2) . . ? O7 C13 C15 116(2) . . ? C16 C13 C15 120(3) . . ? C10B C9 O5 124(3) . . ? C10B C9 C10A 56(2) . . ? O5 C9 C10A 121(2) . . ? C12 C11 O4 108(2) . . ? O8 C14 C16 123(2) . . ? O8 C14 C17 121(3) . . ? C16 C14 C17 117(3) . . ? C6 C5 O3 113(4) . . ? C8 C7 O6 103(4) . . ? C2 C1 O1 124(5) . . ? C10B C10A C9 59(3) . . ? C9 C10B C10A 64(3) . . ? C14 O8 Co1 129.1(15) . . ? C13 C16 C14 127(2) . . ? C3B C4 C3A 63(7) . . ? C3B C3A C4 46(6) . . ? C3B C3A O2 57(6) . . ? C4 C3A O2 83(4) . . ? C4 C3B C3A 72(9) . . ? C4 C3B O2 112(10) . . ? C3A C3B O2 82(8) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.271 _refine_diff_density_min -1.474 _refine_diff_density_rms 0.144 data_taetac6m _database_code_depnum_ccdc_archive 'CCDC 212057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H27 O6 Ta' _chemical_formula_weight 460.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.470(2) _cell_length_b 14.687(4) _cell_length_c 14.815(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.047(5) _cell_angle_gamma 90.00 _cell_volume 1842.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2024(I>2sigma(I)) _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 28.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 5.982 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1982 _exptl_absorpt_correction_T_max 0.2220 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5455 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 19.99 _reflns_number_total 1711 _reflns_number_gt 1014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1711 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.05337(10) 0.68906(5) 0.24994(6) 0.0785(5) Uani 1 1 d . . . O1 O -0.1268(15) 0.6190(8) 0.2517(11) 0.109(5) Uani 1 1 d . . . O6 O 0.1347(19) 0.5906(8) 0.3421(11) 0.117(6) Uani 1 1 d . . . O5 O 0.1395(16) 0.5911(8) 0.1578(9) 0.103(5) Uani 1 1 d . . . O2 O -0.0139(16) 0.7609(9) 0.3490(10) 0.111(5) Uani 1 1 d . . . O3 O -0.0113(16) 0.7593(9) 0.1573(10) 0.108(5) Uani 1 1 d . . . O4 O 0.2553(17) 0.7347(8) 0.2480(10) 0.099(4) Uani 1 1 d . . . C7 C 0.413(4) 0.712(2) 0.238(2) 0.154(11) Uiso 1 1 d . . . H7A H 0.4365 0.6675 0.2843 0.185 Uiso 1 1 calc R . . H7B H 0.4225 0.6814 0.1806 0.185 Uiso 1 1 calc R . . C8 C 0.518(4) 0.768(3) 0.241(2) 0.207(15) Uiso 1 1 d . . . H8A H 0.6183 0.7376 0.2351 0.311 Uiso 1 1 calc R . . H8B H 0.5147 0.7999 0.2974 0.311 Uiso 1 1 calc R . . H8C H 0.5058 0.8106 0.1922 0.311 Uiso 1 1 calc R . . C12 C 0.244(3) 0.4677(18) 0.085(2) 0.182(13) Uani 1 1 d . . . H12A H 0.2965 0.4098 0.0874 0.273 Uiso 1 1 calc R . . H12B H 0.3065 0.5101 0.0514 0.273 Uiso 1 1 calc R . . H12C H 0.1427 0.4606 0.0567 0.273 Uiso 1 1 calc R . . C1 C -0.182(6) 0.530(3) 0.258(4) 0.28(2) Uiso 1 1 d . . . H1A H -0.1425 0.5014 0.2035 0.335 Uiso 1 1 calc R . . H1B H -0.1187 0.5042 0.3066 0.335 Uiso 1 1 calc R . . C5 C -0.101(5) 0.751(3) 0.086(3) 0.235(18) Uiso 1 1 d . . . H5A H -0.0497 0.7025 0.0524 0.282 Uiso 1 1 calc R . . H5B H -0.1965 0.7237 0.1102 0.282 Uiso 1 1 calc R . . C13 C 0.239(4) 0.4694(17) 0.430(2) 0.215(18) Uani 1 1 d . . . H13A H 0.2941 0.4130 0.4217 0.322 Uiso 1 1 calc R . . H13B H 0.1373 0.4577 0.4562 0.322 Uiso 1 1 calc R . . H13C H 0.2985 0.5087 0.4685 0.322 Uiso 1 1 calc R . . C2 C -0.294(6) 0.499(3) 0.267(3) 0.29(2) Uiso 1 1 d . . . H2A H -0.2804 0.4399 0.2946 0.431 Uiso 1 1 calc R . . H2B H -0.3452 0.4919 0.2099 0.431 Uiso 1 1 calc R . . H2C H -0.3578 0.5362 0.3060 0.431 Uiso 1 1 calc R . . C6 C -0.145(6) 0.799(3) 0.032(4) 0.31(3) Uiso 1 1 d . . . H6A H -0.2135 0.7669 -0.0086 0.467 Uiso 1 1 calc R . . H6B H -0.0571 0.8235 -0.0009 0.467 Uiso 1 1 calc R . . H6C H -0.2026 0.8481 0.0597 0.467 Uiso 1 1 calc R . . C9 C 0.219(3) 0.5062(18) 0.188(3) 0.166(16) Uani 1 1 d . . . C11 C 0.216(4) 0.516(3) 0.337(3) 0.153(17) Uani 1 1 d . . . C10 C 0.225(6) 0.478(3) 0.273(3) 0.24(4) Uani 1 1 d . . . H10A H 0.2381 0.4158 0.2803 0.285 Uiso 1 1 calc R . . C4 C -0.136(7) 0.810(3) 0.468(4) 0.35(3) Uiso 1 1 d . . . H4A H -0.1949 0.8013 0.5223 0.530 Uiso 1 1 calc R . . H4B H -0.1956 0.8467 0.4265 0.530 Uiso 1 1 calc R . . H4C H -0.0375 0.8389 0.4810 0.530 Uiso 1 1 calc R . . C3 C -0.113(5) 0.742(3) 0.436(3) 0.247(19) Uiso 1 1 d . . . H3A H -0.2117 0.7125 0.4210 0.296 Uiso 1 1 calc R . . H3B H -0.0547 0.7036 0.4775 0.296 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.0880(7) 0.0430(5) 0.1044(8) -0.0002(6) 0.0022(5) 0.0032(5) O1 0.081(9) 0.072(8) 0.175(15) 0.002(10) -0.008(10) -0.023(7) O6 0.154(15) 0.045(8) 0.154(15) 0.019(9) -0.033(11) 0.019(9) O5 0.123(12) 0.074(10) 0.112(12) -0.019(8) 0.027(9) 0.021(8) O2 0.121(12) 0.091(9) 0.122(12) -0.024(9) 0.016(10) 0.012(9) O3 0.119(12) 0.102(10) 0.104(11) -0.007(9) -0.032(10) -0.003(9) O4 0.096(11) 0.062(7) 0.138(12) 0.009(9) 0.015(9) -0.010(7) C12 0.16(2) 0.14(2) 0.25(4) -0.03(2) 0.10(2) 0.011(19) C13 0.33(4) 0.11(2) 0.20(3) 0.11(2) -0.06(3) 0.05(2) C9 0.065(16) 0.09(2) 0.34(5) -0.15(3) 0.05(2) 0.004(14) C11 0.10(2) 0.11(3) 0.25(5) -0.04(3) -0.05(3) -0.036(18) C10 0.33(6) 0.15(4) 0.23(5) 0.12(4) -0.19(5) -0.07(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 O3 1.802(14) . ? Ta1 O4 1.837(14) . ? Ta1 O1 1.840(12) . ? Ta1 O2 1.895(14) . ? Ta1 O6 2.104(13) . ? Ta1 O5 2.113(12) . ? O1 C1 1.39(5) . ? O6 C11 1.30(4) . ? O5 C9 1.49(4) . ? O2 C3 1.57(4) . ? O3 C5 1.30(4) . ? O4 C7 1.38(3) . ? C7 C8 1.21(4) . ? C12 C9 1.64(4) . ? C1 C2 1.06(6) . ? C5 C6 1.14(5) . ? C13 C11 1.55(5) . ? C9 C10 1.32(5) . ? C11 C10 1.09(6) . ? C4 C3 1.11(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ta1 O4 93.5(6) . . ? O3 Ta1 O1 94.6(6) . . ? O4 Ta1 O1 167.4(5) . . ? O3 Ta1 O2 100.3(7) . . ? O4 Ta1 O2 95.1(6) . . ? O1 Ta1 O2 92.9(7) . . ? O3 Ta1 O6 170.7(6) . . ? O4 Ta1 O6 87.5(6) . . ? O1 Ta1 O6 83.0(6) . . ? O2 Ta1 O6 88.8(6) . . ? O3 Ta1 O5 90.2(6) . . ? O4 Ta1 O5 85.2(6) . . ? O1 Ta1 O5 85.2(6) . . ? O2 Ta1 O5 169.4(6) . . ? O6 Ta1 O5 80.7(6) . . ? C1 O1 Ta1 143(2) . . ? C11 O6 Ta1 136(2) . . ? C9 O5 Ta1 122.1(17) . . ? C3 O2 Ta1 134.8(19) . . ? C5 O3 Ta1 137(2) . . ? C7 O4 Ta1 144.5(15) . . ? C8 C7 O4 123(3) . . ? C2 C1 O1 135(6) . . ? C6 C5 O3 135(5) . . ? C10 C9 O5 124(3) . . ? C10 C9 C12 141(3) . . ? O5 C9 C12 94(3) . . ? C10 C11 O6 121(5) . . ? C10 C11 C13 122(4) . . ? O6 C11 C13 113(3) . . ? C11 C10 C9 131(5) . . ? C4 C3 O2 107(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 19.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.761 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.131